#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:22:20 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179787 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/83/7008364.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7008364
loop_
_publ_author_name
'Elhaik, Jerome'
'Evans, David J.'
'Kilner, Colin A.'
'Halcrow, Malcolm A.'
_publ_section_title
;
 A structural, magnetic and Mössbauer spectroscopic study of an
 unusual angular Jahn-Teller distortion in a series of high-spin
 iron(II) complexes.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1693
_journal_page_last               1700
_journal_paper_doi               10.1039/b502175h
_journal_year                    2005
_chemical_formula_moiety         'C22 H18 Fe N10, 2[Cl O4]'
_chemical_formula_sum            'C22 H18 Cl2 Fe N10 O8'
_chemical_formula_weight         677.21
_chemical_name_systematic
;
Bis-[2,6-dipyrazol-1-ylpyridine]iron(II) diperchlorate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.4384(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.3860(3)
_cell_length_b                   9.2460(2)
_cell_length_c                   20.1033(4)
_cell_measurement_reflns_used    13839
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.63
_cell_volume                     2637.80(10)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEX (McArdle, 1995)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '/w and /f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            13839
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    0.844
_exptl_absorpt_correction_T_max  0.913
_exptl_absorpt_correction_T_min  0.810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Using multiple and symmetry-related data measurements via the program SORTAV
See R.H. Blessing, Acta Cryst (1995), A51, 33-38
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Rectamgular prism'
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.877
_refine_diff_density_rms         0.205
_refine_ls_extinction_coef       0.0023(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         3013
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0475P)²+3.9495P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1052
_reflns_number_gt                2524
_reflns_number_total             3013
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b502175h.txt
_cod_data_source_block           c:\datasets\leeds\mh87\mh87
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        2637.76(10)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7008364
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.0000 0.69509(4) 0.2500 0.02221(15) Uani 1 2 d S . .
N2 N 0.01443(12) 0.74454(19) 0.35660(8) 0.0225(4) Uani 1 1 d . . .
C3 C -0.03005(14) 0.6655(2) 0.39681(10) 0.0229(4) Uani 1 1 d . . .
C4 C -0.02808(15) 0.6954(2) 0.46449(10) 0.0279(5) Uani 1 1 d . . .
H4 H -0.0627 0.6394 0.4916 0.034 Uiso 1 1 calc R . .
C5 C 0.02697(16) 0.8113(2) 0.49052(11) 0.0310(5) Uani 1 1 d . . .
H5 H 0.0300 0.8363 0.5367 0.037 Uiso 1 1 calc R . .
C6 C 0.07796(16) 0.8920(3) 0.45067(11) 0.0300(5) Uani 1 1 d . . .
H6 H 0.1179 0.9692 0.4688 0.036 Uiso 1 1 calc R . .
C7 C 0.06774(14) 0.8545(2) 0.38342(10) 0.0248(4) Uani 1 1 d . . .
N8 N -0.07716(12) 0.54606(19) 0.36366(8) 0.0236(4) Uani 1 1 d . . .
N9 N -0.06758(12) 0.5215(2) 0.29792(8) 0.0251(4) Uani 1 1 d . . .
C10 C -0.10418(15) 0.3915(2) 0.28340(11) 0.0277(5) Uani 1 1 d . . .
H10 H -0.1078 0.3454 0.2408 0.033 Uiso 1 1 calc R . .
C11 C -0.13716(16) 0.3305(2) 0.33961(11) 0.0299(5) Uani 1 1 d . . .
H11 H -0.1661 0.2387 0.3421 0.036 Uiso 1 1 calc R . .
C12 C -0.11854(15) 0.4312(2) 0.38946(11) 0.0279(5) Uani 1 1 d . . .
H12 H -0.1320 0.4229 0.4340 0.034 Uiso 1 1 calc R . .
N13 N 0.11370(12) 0.92549(19) 0.33611(9) 0.0255(4) Uani 1 1 d . . .
N14 N 0.10695(12) 0.8672(2) 0.27286(9) 0.0262(4) Uani 1 1 d . . .
C15 C 0.15616(15) 0.9567(2) 0.24009(11) 0.0295(5) Uani 1 1 d . . .
H15 H 0.1644 0.9444 0.1945 0.035 Uiso 1 1 calc R . .
C16 C 0.19418(16) 1.0715(3) 0.28128(12) 0.0326(5) Uani 1 1 d . . .
H16 H 0.2319 1.1487 0.2694 0.039 Uiso 1 1 calc R . .
C17 C 0.16578(16) 1.0493(2) 0.34197(12) 0.0314(5) Uani 1 1 d . . .
H17 H 0.1796 1.1088 0.3809 0.038 Uiso 1 1 calc R . .
Cl18 Cl 0.29743(4) 0.95837(7) 0.08946(3) 0.03291(18) Uani 1 1 d . . .
O19 O 0.21843(16) 0.8670(3) 0.09178(12) 0.0763(8) Uani 1 1 d . . .
O20 O 0.38256(14) 0.8765(2) 0.10612(9) 0.0470(5) Uani 1 1 d . . .
O21 O 0.29790(15) 1.0723(2) 0.13840(12) 0.0561(6) Uani 1 1 d . . .
O22 O 0.29469(17) 1.0166(4) 0.02358(11) 0.0870(10) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 155.65(10) . 2 ?
N2 Fe1 N9 72.29(6) . . ?
N2 Fe1 N9 127.92(6) 2 . ?
N9 Fe1 N9 85.24(9) 2 . ?
N2 Fe1 N14 72.05(6) . . ?
N2 Fe1 N14 90.24(6) 2 . ?
N9 Fe1 N14 106.03(6) 2 . ?
N9 Fe1 N14 141.63(6) . . ?
N14 Fe1 N14 87.83(10) . 2 ?
C3 N2 C7 118.41(17) . . ?
C3 N2 Fe1 120.52(14) . . ?
C7 N2 Fe1 121.07(13) . . ?
N2 C3 C4 123.6(2) . . ?
N2 C3 N8 112.73(17) . . ?
C4 C3 N8 123.63(19) . . ?
C5 C4 C3 116.4(2) . . ?
C4 C5 C6 121.45(19) . . ?
C7 C6 C5 116.6(2) . . ?
N2 C7 C6 123.3(2) . . ?
N2 C7 N13 112.67(17) . . ?
C6 C7 N13 124.0(2) . . ?
C12 N8 N9 110.98(17) . . ?
C12 N8 C3 129.75(17) . . ?
N9 N8 C3 118.08(16) . . ?
C10 N9 N8 105.28(16) . . ?
C10 N9 Fe1 139.45(14) . . ?
N8 N9 Fe1 115.28(13) . . ?
N9 C10 C11 111.07(19) . . ?
C12 C11 C10 105.29(19) . . ?
N8 C12 C11 107.39(18) . . ?
C17 N13 N14 111.42(18) . . ?
C17 N13 C7 130.26(19) . . ?
N14 N13 C7 118.31(17) . . ?
C15 N14 N13 104.58(18) . . ?
C15 N14 Fe1 138.91(15) . . ?
N13 N14 Fe1 114.69(12) . . ?
N14 C15 C16 111.5(2) . . ?
C17 C16 C15 105.6(2) . . ?
N13 C17 C16 106.9(2) . . ?
O19 Cl18 O22 110.76(17) . . ?
O19 Cl18 O20 109.61(16) . . ?
O22 Cl18 O20 108.03(12) . . ?
O19 Cl18 O21 109.04(12) . . ?
O22 Cl18 O21 110.78(17) . . ?
O20 Cl18 O21 108.60(13) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.1676(16) . ?
Fe1 N9 2.1808(18) . ?
Fe1 N14 2.2085(18) . ?
N2 C3 1.329(3) . ?
N2 C7 1.333(3) . ?
C3 C4 1.384(3) . ?
C3 N8 1.406(3) . ?
C4 C5 1.383(3) . ?
C5 C6 1.389(3) . ?
C6 C7 1.380(3) . ?
C7 N13 1.407(3) . ?
N8 C12 1.361(3) . ?
N8 N9 1.370(2) . ?
N9 C10 1.326(3) . ?
C10 C11 1.413(3) . ?
C11 C12 1.362(3) . ?
N13 C17 1.363(3) . ?
N13 N14 1.370(2) . ?
N14 C15 1.332(3) . ?
C15 C16 1.401(3) . ?
C16 C17 1.364(3) . ?
Cl18 O19 1.423(2) . ?
Cl18 O22 1.424(2) . ?
Cl18 O20 1.4320(19) . ?
Cl18 O21 1.441(2) . ?
